静态顶空/气相色谱-质谱法同时测定化妆品中22种有毒挥发性有机溶剂残留  

Simultaneous Determination of 22 Toxic Volatile Organic Solvent Residues in Cosmetics by Static Headspace/Gas Chromatography-Mass Spectrometry

作　　者：车文军 沈珺[2] 王燕芹[3] 王小丹 浦婕 

机构地区：[1]苏州世谱检测技术有限公司,江苏苏州215123 [2]苏州卫生职业技术学院药学院,江苏苏州215009 [3]南京林业大学理学院,江苏南京210037

出　　处：《分析测试学报》2017年第5期697-700,共4页Journal of Instrumental Analysis

摘　　要：以2015版《化妆品安全技术规范》中规定的常见禁用及限用有毒挥发性有机溶剂为研究对象,建立了静态顶空/气相色谱-质谱法(SHS/GC-MS)同时测定化妆品中22种有毒挥发性有机溶剂(VOC)(二氯甲烷、顺式-1,2-二氯乙烯、反式-1,2-二氯乙烯、2-氯-1,3-丁二烯、三氯甲烷、1,2-二氯乙烷、苯、四氯化碳、三氯乙烯、甲苯、四氯乙烯、氯苯、乙苯、三溴甲烷、间二甲苯、对二甲苯、苯乙烯、邻二甲苯、异丙苯、1,4-二氯苯、1,2-二氯苯、六氯丁二烯)残留的检测方法。试样在80℃下30 min静态顶空,经DB-1柱分离后,采用选择离子监测模式(SIM)进行定性定量分析。优化了顶空、色谱和质谱参数,结果表明:22种VOC在0.5~50 ng/m L浓度范围内均呈良好的线性关系,相关系数均大于0.99,在1.0,2.0,5.0 ng/m L 3个浓度加标水平下的平均回收率为80.3%~102.7%,相对标准偏差(RSD,n=6)为6.4%~9.9%,检出限为0.2~5.0 ng/g。结果表明,该方法简便、灵敏、准确,具有良好的重现性和稳定性,适合于化妆品中22种VOC残留的筛查和确证检测。Based on the Safety and Technical Standards for Cosmetics（2015）, a staticheadspace/gas chromatography- mass spectrometric （SHS/GC -MS） method was established to analyze 22 volatile organic compounds（VOCs） residues, including diehloromethane, cis-1,2-dichloroethene, trans-1, 2-dichloroethylene, 2-chloro-1,3-butadiene, trichloromethane, 1,2-dichloroethane, benzene, carbon tetrachloride, trichloroethylene, methylbenzene, tetrachloroethylene, chlorobenzene, ethyl- benzene, tribromomethane, m-xylene, p-xylene, phenylethylene, o-xylene, isopropylbenzene, 1, 4-dichlorobenzene, 1,2-diehlorobenzene and hexachlorobutadiene in cosmetics. The experimental conditions for SHS/GC - MS, such as headspace conditions, analytical conditions of GC, quantita- tive ion＇s selection and concentration of the samples were optimized. The cosmetic samples were extracted and cleaned-up by headspace at 80℃ for 30 min, determined and quantified by MS. 22 kinds of VOCs had good linear relations in the range of 0. 5 - 50 ng/mL with correlation coefficients higher than 0.99. The spiked recoveries ranged from 80. 3% to 102.7% , with relative standard deviations （RSD） of 6.4% - 9.9% . The limits of detection were in the range of 0. 2 - 5.0 ng/g. This method had the advantages of simplicity, sensitivvity, accurancy, good reproducibility and stability, and was suitable for the screening and analysis of VOCs residues in cosmetics.

关 键 词：静态顶空 气相色谱-质谱(GC—MS) 化妆品 挥发性有机溶剂 测定 

分 类 号：O657.71[理学—分析化学] TQ047.8[理学—化学]